Tetrabutylammonium Fluoride → 1-(1,4-dioxa-spiro[4.5]dec-8-yl)-1H-[1,2,3]triazole

HRID 2099685노트

반응식

HRID 2099685 반응식
[O:1]1[C:5]2([CH2:10][CH2:9][CH:8]([N:11]3[CH:15]=[C:14]([Si](C)(C)C)[N:13]=[N:12]3)[CH2:7][CH2:6]2)[O:4][CH2:3][CH2:2]1.[F-].C([N+](CCCC)(CCCC)CCCC)CCC>C1COCC1.CCOC(C)=O>[O:1]1[C:5]2([CH2:10][CH2:9][CH:8]([N:11]3[CH:15]=[CH:14][N:13]=[N:12]3)[CH2:7][CH2:6]2)[O:4][CH2:3][CH2:2]1

참가 물질

5

반응물 2

HCID 2724141Tetrabutylammonium FluorideHCID 577954251-(1,4-dioxa-spiro[4.5]dec-8-yl)-4-trimethylsilanyl-1H-[1,2,3]triazole

생성물 1

HCID 574240951-(1,4-dioxa-spiro[4.5]dec-8-yl)-1H-[1,2,3]triazole수율 89.1%

시약·촉매·용매 2

HCID 8028Tetrahydrofuran용매2회HCID 8857Ethyl Acetate용매

실험 절차

A solution of 1-(1,4-dioxa-spiro[4.5]dec-8-yl)-4-trimethylsilanyl-1H-[1,2,3]-triazole (1.60 g, 5.68) in 41 mL of dry THF was treated by a 1M solution of tetrabutylammonium fluoride in THF (9.0 mL, 9.0 mmol). The resulting mixture was stirred for 48 h at room temperature under nitrogen. It was diluted with EtOAc, washed with saturated aqueous ammonium chloride, water and brine, dried over Na2SO4 and concentrated to give 1-(1,4-dioxa-spiro[4.5]dec-8-yl)-1H-[1,2,3]triazole (1.06 g, 89%).

후처리

  1. washwashed with saturated aqueous ammonium chloride, water and brine
  2. dry with materialdried over Na2SO4
  3. concentrationconcentrated

출처 및 근거

ORD 기록
ord-2ad7a1f071d2457c8ec436a04585e5ab
출처 데이터셋
uspto-grants-2009_08
특허 번호
US07569600B2

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